Low-odor, higher molecular weight polyether polyols are produced by purifying the polyether polyols at temperatures of 110° to 150°C and pressures of 10 to 70 hPa with the addition of 5 to 30% by weight of water, wherein the water is passed in finely divided form, with a droplet diameter of about 5 to 100 μ, through the polyether polyols to be purified for a time of metered addition of 1 to 5 hours.
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1. In a process for the production of a polyurethane comprising reacting a polyisocyanate with an isocyanate-reactive component via the polyisocyanate polyaddition process, the imporvement wherein said isocyanate reactive component comprises a low-odor, monofunctional or polyfunctional polyether polyol having a molecular weight of from about 750 to 18,000, and a viscosity at 25°C of about 40 to 25,000 mPa.s, made by the process comprising
1) purifying polyether polyol at temperatures of about 100° to 150°C and at pressures of about 10 to 70 hPa, wherein about 5 to 30.0% by weight of water, based on the quantity of polyether polyol present, is metered into said polyether polyol over a time period of about 1 hour up to about 5 hours, said water being in finely divided form and having a droplet diameter of 5 to 100μ,
wherein the resultant polyether polyol contains a) less than about 1.5 ppm of 2-methyl-2-pentenal, b) less than about 1.0 ppm of allyl alcohol, c) less than about 15 ppm of allyloxypropanol, d) less than about 50 ppm of dipropylene glycol allyl ether, and e) less than about 1.0 ppm of propionaldehyde. 2. The process of
3. The process of
4. The process of
5. The process of
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The invention is further illustrated but is not intended to be limited by the following examples in which all parts and percentages are by weight unless otherwise specified.
In the following examples, 1000 g of various polyether polyols (as described below) were heated to 120°C 200 g water (20% by weight) were introduced at a pressure of 18 hPa via thin inlet tubes (diameter 0.2 mm) at a rate such that the temperature did not fail below 120°C and the pressure did not rise above 40 hPa. The water was added to the unpurified polyether polyols over a time period of 3 hours. The water vapor bubbles had an average diameter of 7 to 50μ. Di- and trifunctional PO- and PO/EO polyethers were used in the examples. The effect of the purification according to the invention on the impurities in the polyether polyols used is apparent from Table 1. It can clearly be seen that after purification, the unwanted by-products, which amongst other effects resulted in the formation of an odor, were very extensively removed. Analysis was performed by means of head-space gas chromatography.
Polyether polyol 1: a glycerine started ethylene oxide/propylene oxide polyether which is branched, having an OH number of about 46, a molecular weight of about 3660 and a viscosity of about 560 mPa.s.
Polyether polyol 2: a propylene glycol started propylene oxide polyether which is linear, having an OH number of about 112, a molecular weight of about 1000 and a viscosity of about 140 mPa.s.
Polyether polyol 3: a propylene glycol started propylene oxide polyether which is linear, having an OH number of about 56, a molecular weight of about 2000 and a viscosity of about 310 mPa.s.
Polyether polyol 4: a trimethylolpropane started propylene oxide/ethylene oxide polyether which is branched, having an OH number of about 28, a molecular weight of about 6000 and a viscosity of about 1120 mPa.s.
TABLE 1 |
______________________________________ |
Example 1 Example 2 |
Polyether polyol 1 |
Polyether polyol 2 |
before after before after |
Compounds in the |
purifica- |
purifica- |
purifica- |
purifica- |
polyether polyols |
tion tion tion tion |
______________________________________ |
1,4-dioxan <0,1 <0,1 <0,1 <0,1 |
2,4-dimethyl-1,3- |
1,5 <0,1 <0,1 <0,1 |
dioxolane |
2-ethylene-4-methyl- |
2,5 <0,1 <0,1 <0,1 |
1,3-dioxolone |
2-methyl-2-pentenal |
1,8 <0,1 2,2 <0,1 |
acetaldehyde 1,2 0,1 1,9 2 |
allyl alcohol |
<0,1 <0,1 0,6 <0,1 |
allyl oxypropanol |
80 <0,1 0,6 <0,1 |
butyraldehyde |
<0,1 <0,1 <0,1 <0,1 |
DPG allyl ether |
460 <0,1 480 <0,1 |
propionaldehyde |
1,1 0,1 0,4 0,3 |
sum of unknown |
20 8 15 8 |
readily volatile |
compounds |
______________________________________ |
(all data in ppm) |
TABLE 2 |
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Example 3 Example 4 |
before after before after |
Compounds in the |
purifica- |
purifica- |
purifica- |
purifica- |
polyether polyols |
tion tion tion tion |
______________________________________ |
1,4-dioxan <0,1, <0,1 <0,1 <0,1 |
2,4-dimethyl-1,3- |
<0,1 <0,1 <0,1 <0,1 |
dioxolane |
2-ethylene-4-methyl- |
1,2 <0,1 <0,1 <0,1 |
1,3-dioxolone |
2-methyl-2-pentenal |
6 0,3 0,3 <0,1 |
acetaldehyde 0,5 0,8 0,6 1,3 |
allyl alcohol |
1,8 <0,1 <0,1 <0,1 |
allyl oxypropanol |
170 1,4 12 0,3 |
butyraldehyde |
<0,1 <0,1 <0,1 <0,1 |
DPG allyl ether |
650 <0,1 55 <0,1 |
propionaldehyde |
2,7 0,1 0,3 0,3 |
sum of unknown |
8 8 8 4 |
readily volatile |
compounds |
______________________________________ |
(all data in ppm) |
Although the invention has been described in detail in the foregoing for the purpose of illustration, it is to be understood that such detail is solely for that purpose and that variations can be made therein by those skilled in the art without departing from the spirit and scope of the invention except as it may be limited by the claims.
Jacobs, Gundolf, Gupta, Pramod, Leuridan, Joel
Patent | Priority | Assignee | Title |
Patent | Priority | Assignee | Title |
3653183, | |||
4143072, | Dec 10 1977 | Bayer Aktiengesellschaft | Process for the purification of polyethers using a tubular coil evaporator |
5248794, | Feb 16 1993 | The Dow Chemical Company | Process for purifying propylene oxide |
JP56104936, |
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